The major processes for introducing polycyclic aromatic hydrocarbons (PAHs) in food are smoking and grilling of different products. But in addition, PAHs can permeate in the food chain due to their high lipophilicity and ability to be accumulated in specific tissue, through contaminated animal feed. Further, when some parts of these animals are marketed as food, the accumulated PAHs can go to the human organism. Some of them are classified as highly toxic, carcinogenic and mutagenic for animal and human organisms so they are under consideration of International and European legislation. This work reports development and validation of simple and fast GC/MS method for 16 PAHs determination. Comparison of two methods for sample preparation in pork meat matrix standard extraction/saponification procedure and modified QuEChERS method is also done. In addition, this paper report the calibration step of instrument and a recovery study for 16 PAHs in model pork meat, using modified QuEChERS procedure for sample pretreatment. The calibration step with accessible and suitable for use in real laboratory conditions internal standard (chrysene D12) is done in the range 10–100 ppb using toluene as solvent. The obtained results show very good linearity (R2 = 0.99 to 1.00). For the recovery study six model samples were spiked with 16 PAHs and they all are subjected to QuEChERS procedure. The recovery is calculated and the obtained data (71–120%) is in a good correlation with requirements of international legislation. Finally, LOD values for all 16 investigated compounds of modified GC/MS method and for the instrument were determined.
The authorities have identified an emerging trend where over-the-counter products, represented as dietary supplements, contain hidden active ingredients that could be harmful. Consumers may unknowingly take products laced with varying quantities of approved prescription drug ingredients, controlled substances, and untested and unstudied pharmaceutically active ingredients. Hidden ingredients are increasingly becoming a problem in products promoted for sexual enhancement, weight loss, or bodybuilding. The tests have revealed the presence of some undesired substances like sildenafil, tadalafil, vardenafil, and their analogues in tainted sexual enhancement products. The content of these substances is usually around the daily curative dose. A simple high-performance liquid chromatography (HPLC) method for simultaneously determination of sildenafil, vardenafil, tadalafil, dapoxetine, yohimbine, and sibutramine was developed and validated. InfinityLab Poroshell 120 EC-C18 (150 '4.6 mm '4 μm particles) was used, as well as a diode-array detector (DAD) at 230 nm, and a gradient flow with 0.030 М ammonium acetate buffer and acetonitrile. The method is linear in the following range: 2.5–37.5 μg/mL for yohimbine, 2.06–30.9 μg/mL for vardenafil, 2.0–30.0 μg/mL for sildenafil, 3.1–46.5 μg/mL for tadalafil, 1.98–29.7 μg/mL for dapoxetine, and 2.2–66.0 μg/mL for sibutramine. The linearity coefficient is R2 = 1 for all substances. Model matrices were spiked, and the analytical recoveries for all substances are in the range 97.5%–99.5%. The method exhibited an upper hand compared with previously reported methods in terms of speed and simplicity. Additionally, the mobile phase (also used as extracting, column washing, and diluting solvent) was composed of only buffer and acetonitrile, which rendered the method much cheaper than others.